Method of preparing antimony sulphide



Patented May 29, 1928.

warren sr 'r s PATENT OFFICE.

HANS NUI-IN, OF KARLSR'UHE, GERMANY, AND LEWIS H. BLOOD, OE MATAWAN, NEW JERSEY, ASSIGNORS To ANTIMONY PRODUCTS CORPORATION, OF NEW YO K,N. 7.,

' A CORPORATION OF DELAWARE.

METHOD OE PREPARING ANTIMONY SULPHID'E,

NO Drawing.

our invention relates to a method; of preparing antimony sulphide by the direct reaction of-sodium sulphide, stibnite and sulphur, produced in an economical and highly eflicientmanner, whereby the difficulties 1nherentin the methods, pursued heretofore are obviated, the expensive andcumbersonie apparatus,heretofore used is dispensed with and the product is manufactured 1n a convenient and inexpensive manner.

We are also enabled to "produce at the same time by-products which are capable of equiyocal use in producing other desirable compounds and avoid the production olibyproducts of little or no value as is the case in the methods heretofore employed.

Prior to our invention, antimony sulphide has been produced commercially, genand sulphur yielding calcium thio-antimonate which is filtered off and precipitated with sulphuric acid yielding antimony penta-sulphide and calcium sulphate.

2. By digesting lime, sulphur, sodium carbonate and stibnite to form a. mixture of sodium and calcium thio-antinionate, which is treated in the manner described in process No. 1, giving calcium sulphate and sodium sulphate and antimony pentasulphide.

8. By fusing sodium carbonate, stibnite and sulphur, leaching with water, filtering and precipitating with sulphuric acid yielding antimony pentasulphide.

All of these processes involve the provision of bulky apparatus which is diflicult of manipulation. All of them involve the production of a large quantity of hydrogen'sulphide and in none of them are the by-prodnets of any substantial value. All of these prior processes require considerable time and the yield is frequently a product which is more or less impure, being adulterated with calcium sulphate.

In our improved process, the apparatus required is simple and easily handled, the

process is a rapid one, involves the formation of no objectionable gases and yields a i Application filed July 27,

1922. Serial No. 578,003.

product substantially the only impurity in by-product sodium thio-sulphate, which may advantageously be used in the formation of antimony oxy-sulphide', or antimony crim- SOII. c i

The following is an example of the manner in which our improved process may be practised, it being understood that the following description is given merely by way of. example of a method that we have found to produce gOOd results and that we do not intend to limit ourselves to the particular proportions or ingredients specified. y

We take one hundred and eightysix pounds-(186 lbs.) of anhydrous sodium sulphide, two hundred and eighty pounds (280 lbs.) of pure stibnite ore (QOO-mesh) and thirty-two pounds (32 lbs.) of sulphur. To these we add approximately fifty gallons of water and digest at boiling temperature for a period of approximately two hours. We then add sufiicient water to bring the solution to 19 Baum and atomize the solution thus formed into a closed chamber. Said chamber is provided with one or more atomizing nozzles through which the solution is driven in any suitable manner, such as by means of steam or compressed air, or by suitable pressure without the admixture of any other fluid. The chamber is also provided with an inlet for sulphur dioxide gas, a slight excess of which is introduced througl'i said inlet and with an outlet for any excess of sulphur dioxide not used in the reaction and for such air or other agent as may be used in introducing the liquid into the chamber. An outlet is provided at the bottom of the chamber through which the product of reaction may be drawn off. We have not illustrated said chamber because it may take a variety offorms, it being only necessary i any other suitable manner, as for instance bu is up ling the sulphur dioxide gas through thesolution, although thismet'hod of procedure requires considerably more 2 time than that described above and requires the provision of a tankfor handling larger quantities of solution for a relatively longer period.

The mixture oi? the liquid ,and the sulphur dioxide reacts .to form antimony pentasulphide, free sulphur and sodium thiosulphate, the sodium thiossulphate remaining in solution and the antimony pentasuh phide being in suspension in the solution. The liquid carrying the-antimony pentas-ulphide in suspension isdnawn ofi' and the solid constituents are separated from the liquid by filtration, or; otherwise.

or-evaporated-to dryness, as desired, de-

pending uponthe use to whiclrthe sodium thio-sulphate is to he put. Theantimony pentasul hide mixed :with the sulphur is dried, it desired, pulverized in asuitable mill and is then ready for use inth e rubber industry.

The reactions are probably the following:

trate is then pumpedinto a separate tank the foregoing being the reaction which occurs during digestion and before atomizatlon as described above.

this being the reaction Which occurs in the atomizing' chamber.

The by-product sodium ethic-sulphate is used in the production of antim'0nycrimson from antimony trichlorideas followsz.

It will beobserved that in the last ream tion a considerable quantity of sulphur dioxide gas is formed, which may be used in reaction 11 above.

mony pentasulphide and antimonycrimson in the same factory, since the sodium'thiosulphate produced as a by-product 1n reaction II may be used in reaction III andthe sulphur dioxide produced as a byproduct in reaction III may be used in reaction II.

What We claim is: v o The step in the method of'makinganti- .mony pentasulphide which comprises atomizing by steam a solution of thio-antimomate and or an acid gas.

In testimony whereof, We have signed our names to this specification'the 26th day of June, 1922, and the 18th day of May,

1922, respectively. H

' HANS, NUHN.

LEWIS H. BLOOD.

Great economies therefore result irom the manuiacture'of anti-- 

